CN109734109B - A kind of method for preparing ethyl xanthate intercalated magnesium aluminum hydrotalcite - Google Patents
A kind of method for preparing ethyl xanthate intercalated magnesium aluminum hydrotalcite Download PDFInfo
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Abstract
本发明公开了一种制备乙基黄原酸插层镁铝水滑石的方法，包括以下步骤：A、将六水合氯化铝与六水合氯化镁按照摩尔比2∶1的比例进行称取溶解，得到混合溶液A；B、将尿素与乙基黄原酸钠按照摩尔比4∶1的比例进行称取溶解，得到混合溶液B；C、将混合溶液B放置在反应容器内，将混合溶液A逐渐滴加至混合溶液B中，与此同时对混合溶液B进行搅拌，在混合溶液A滴加至其总量的50％时，在滴加混合溶液A的同时向混合溶液B中滴加氢氧化钠溶液；D、滴加完毕后加快搅拌速度，持续搅拌2h，然后静置12h；E、将静置后的溶液进行抽滤、干燥、研磨，得淡黄色粉末状水滑石。本发明能够改进现有技术的不足，改善了乙基黄原酸插层镁铝水滑石的晶体结构。
The invention discloses a method for preparing ethylxanthate intercalated magnesium-aluminum hydrotalcite, comprising the following steps: A. Weighing and dissolving aluminum chloride hexahydrate and magnesium chloride hexahydrate in a molar ratio of 2:1; Obtain mixed solution A; B, urea and sodium ethyl xanthate are weighed and dissolved according to the molar ratio of 4:1 to obtain mixed solution B; C, mixed solution B is placed in the reaction vessel, mixed solution A is It is gradually added dropwise to the mixed solution B while stirring the mixed solution B. When the mixed solution A is added dropwise to 50% of its total amount, hydrogen is added dropwise to the mixed solution B while the mixed solution A is added dropwise. Sodium oxide solution; D. After the dropwise addition, increase the stirring speed, continue stirring for 2h, and then stand for 12h; E. Filter, dry and grind the solution after standing to obtain light yellow powdery hydrotalcite. The invention can improve the deficiencies of the prior art and improve the crystal structure of the ethyl xanthate intercalated magnesium-aluminum hydrotalcite.
Description
Technical Field
The invention relates to the technical field of hydrotalcite, in particular to a method for preparing ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite.
Background
Hydrotalcite is an inorganic material with anion lamellar function, has changeable chemical components and performance, and is widely applied to various fields of insulation, flame retardance, ageing resistance and the like of various materials. Magnesium aluminum hydrotalcite is a common hydrotalcite. The ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite is modified magnesium-aluminum hydrotalcite and can provide the antioxidant protection effect of the magnesium-aluminum hydrotalcite. The ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite is generally prepared by a traditional double-drop coprecipitation method. However, the crystal structure of the intercalated magnesium-aluminum hydrotalcite prepared by the method is loose, so that the protective effect of the intercalated magnesium-aluminum hydrotalcite is unsatisfactory.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite, which can overcome the defects of the prior art and improve the crystal structure of the ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A method for preparing ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite comprises the following steps:
A. weighing aluminum chloride hexahydrate and magnesium chloride hexahydrate according to the molar ratio of 2: 1, and then adding the weighed materials into deionized water for dissolving to obtain a mixed solution A;
B. weighing urea and sodium ethyl xanthate according to the molar ratio of 4: 1, and then adding the urea and the sodium ethyl xanthate into deionized water for dissolving to obtain a mixed solution B;
C. placing the mixed solution B in a reaction container, gradually dropwise adding the mixed solution A into the mixed solution B, stirring the mixed solution B at the same time, linearly increasing the temperature in the reaction container from 25 ℃ at the beginning of dropwise adding to 75 ℃ at the end of dropwise adding, dropwise adding a sodium hydroxide solution into the mixed solution B while dropwise adding the mixed solution A when the mixed solution A is dropwise added to 50% of the total amount of the mixed solution A, finishing dropwise adding of the sodium hydroxide solution and the mixed solution A at the same time, wherein the molar ratio of the dropwise added sodium hydroxide to the dropwise added urea is 1: 10;
D. accelerating the stirring speed after the dropwise adding is finished, continuously stirring for 2 hours, and then standing for 12 hours;
E. and (3) carrying out suction filtration on the solution after standing, washing a filter cake to be neutral by using deionized water, drying for 12h at the temperature of 80 ℃, taking out the filter cake, and grinding to obtain light yellow powdery hydrotalcite, namely the ethyl xanthic acid intercalation magnalium hydrotalcite.
Preferably, the molar ratio of the aluminum chloride to the deionized water in the mixed solution A is 2: 25, and the molar ratio of the sodium ethyl xanthate to the deionized water in the mixed solution B is 1: 40.
Preferably, in step C, the stirring speed is 120 rad/min; in step D, the stirring speed is 350 rad/min.
Preferably, in step D, the temperature of the solution at rest is maintained at 40 ℃.
Preferably, in step C and step D, the reaction vessel is purged with nitrogen for protection.
Preferably, the reaction vessel comprises a cavity, an inclined plane is arranged at the bottom of the cavity, the left side end of the inclined plane is higher than the right side end of the inclined plane, a dropping pipe is installed above the left side end of the inclined plane, the tail end of the dropping pipe is connected with a plurality of dropping heads which are arranged side by side, and a stirring paddle is installed above the right side end of the inclined plane.
Preferably, the side wall of the dropping pipe is provided with a first heater, and the inclined surface is internally provided with a second heater.
Adopt the beneficial effect that above-mentioned technical scheme brought to lie in: the invention adopts a urea decomposition precipitation method to prepare the ethyl xanthic acid intercalation magnalium hydrotalcite. On the basis, excessive urea and sodium ethylxanthate solution are adopted in the early stage of reaction, strong base is added in the late stage of reaction, the reaction temperature is changed, and the decomposition rate of urea is gradually increased, so that the crystallinity is improved, and the crystal structure is improved. In the initial stage of crystallization and precipitation, the crystal nucleus can be more uniform by stirring at a low speed; in the later stage of crystallization and precipitation, the crystallization speed can be accelerated by rapid stirring, and the overall consistency of crystal grains is improved. In order to further improve the uniformity of the crystallization reaction, the invention specially designs a reaction container, the bottom of which is an inclined plane, the mixed solution is dripped at the higher end, the solution is quickly mixed by utilizing the height difference, and then the mixed solution is stirred at the lower end (the main area of the crystallization reaction), so that the stirring effect of the stirring process on the crystallization reaction area can be improved.
Drawings
Fig. 1 is an XRD pattern of an ethylxanthic acid intercalated magnesium aluminum hydrotalcite prepared according to an embodiment of the present invention and a comparative example.
Fig. 2 is an SEM image of ethyl xanthate intercalated magnesium aluminum hydrotalcite prepared in one embodiment of the present invention.
Fig. 3 is an SEM image of the ethyl xanthate intercalated magnesium aluminum hydrotalcite prepared in the comparative example.
FIG. 4 is a schematic diagram of a reaction vessel according to an embodiment of the present invention.
FIG. 5 is a structural view of a dropping head in one embodiment of the present invention.
Detailed Description
One embodiment of the present invention comprises the steps of:
A. weighing aluminum chloride hexahydrate and magnesium chloride hexahydrate according to the molar ratio of 2: 1, and then adding the weighed materials into deionized water for dissolving to obtain a mixed solution A;
B. weighing urea and sodium ethyl xanthate according to the molar ratio of 4: 1, and then adding the urea and the sodium ethyl xanthate into deionized water for dissolving to obtain a mixed solution B;
C. placing the mixed solution B in a reaction container, gradually dropwise adding the mixed solution A into the mixed solution B, stirring the mixed solution B at the same time, linearly increasing the temperature in the reaction container from 25 ℃ at the beginning of dropwise adding to 75 ℃ at the end of dropwise adding, dropwise adding a sodium hydroxide solution into the mixed solution B while dropwise adding the mixed solution A when the mixed solution A is dropwise added to 50% of the total amount of the mixed solution A, finishing dropwise adding of the sodium hydroxide solution and the mixed solution A at the same time, wherein the molar ratio of the dropwise added sodium hydroxide to the dropwise added urea is 1: 10;
D. accelerating the stirring speed after the dropwise adding is finished, continuously stirring for 2 hours, and then standing for 12 hours;
E. and (3) carrying out suction filtration on the solution after standing, washing a filter cake to be neutral by using deionized water, drying for 12h at the temperature of 80 ℃, taking out the filter cake, and grinding to obtain light yellow powdery hydrotalcite, namely the ethyl xanthic acid intercalation magnalium hydrotalcite.
In the mixed solution A, the molar ratio of aluminum chloride to deionized water is 2: 25, and in the mixed solution B, the molar ratio of sodium ethyl xanthate to deionized water is 1: 40.
In step C, the stirring speed is 120 rad/min; in step D, the stirring speed is 350 rad/min.
In step D, the temperature of the solution at the time of standing was maintained at 40 ℃.
And in the step C and the step D, nitrogen is filled into the reaction container for protection.
Referring to fig. 4-5, the reaction vessel includes a cavity 1, a slope 2 is provided at the bottom of the cavity 1, the left side end of the slope 2 is higher than the right side end, a dropping pipe 3 is installed above the left side end of the slope 2, the end of the dropping pipe 3 is connected with a plurality of dropping heads 4 arranged side by side, and a stirring paddle 7 is installed above the right side end of the slope 2. The side wall of the dropping pipe 3 is provided with a first heater 8, and the inclined plane 2 is internally provided with a second heater 9.
In addition, a necking part 5 is arranged in the dropping head 4, and a tooth-shaped part 6 is arranged at the bottom edge of the dropping head 4. The structure of the dripping head can enlarge the diameter of liquid drops in the dripping process, thereby improving the mixing speed of the liquid after the liquid drops into the mixed solution.
Comparative example (double drop coprecipitation method)
(1) Weighing a certain amount of magnesium salt and aluminum salt according to the Mg/Al molar ratio of 3: 1, and adding 100ml of deionized water for complete dissolution to obtain a uniform mixed salt solution;
(2) weighing a certain amount of NaOH and sodium ethyl xanthate (C2H5OCS2Na) in a beaker according to the ratio of n (OH-) (Mg2+ + Al3+) (2: 1) to n (Al3+) (C2H5OCS2-) (1: 1), and adding 100ml of deionized water to completely dissolve the NaOH and the sodium ethyl xanthate (C2H5OCS2Na) to obtain a uniform mixed alkali solution;
(3) cleaning and drying two constant-pressure funnels with good air tightness and the same specification, and respectively transferring the mixed salt and the alkali solution into the constant-pressure funnels;
(4) slowly dripping the mixed salt and the alkali solution in the constant-pressure funnel into a beaker, stirring at a constant speed, and adjusting the titration speed to ensure that the pH of the reaction system is always more than 10;
(5) continuously stirring for 2 hours at room temperature after the dropwise addition is finished;
(6) after stirring, placing the beaker in a constant-temperature water bath box, crystallizing for a certain time at a certain temperature, and taking out, wherein the lower part of the beaker is a faint yellow precipitate;
(7) carrying out suction filtration on the aged solution, washing a filter cake to be neutral by using deionized water, and drying at 80 ℃ for 12 hours;
(8) and taking out the filter cake, and grinding to obtain light yellow powdery hydrotalcite, namely the ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite.
Referring to fig. 1-3, the ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite prepared by the invention has a better crystal structure.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The method for preparing the ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite is characterized by comprising the following steps of:
A. weighing aluminum chloride hexahydrate and magnesium chloride hexahydrate according to the molar ratio of 2: 1, and then adding the weighed materials into deionized water for dissolving to obtain a mixed solution A;
B. weighing urea and sodium ethyl xanthate according to the molar ratio of 4: 1, and then adding the urea and the sodium ethyl xanthate into deionized water for dissolving to obtain a mixed solution B;
C. placing the mixed solution B in a reaction container, gradually dropwise adding the mixed solution A into the mixed solution B, stirring the mixed solution B at the same time, linearly increasing the temperature in the reaction container from 25 ℃ at the beginning of dropwise adding to 75 ℃ at the end of dropwise adding, dropwise adding a sodium hydroxide solution into the mixed solution B while dropwise adding the mixed solution A when the mixed solution A is dropwise added to 50% of the total amount of the mixed solution A, and finishing dropwise adding of the sodium hydroxide solution and the mixed solution A at the same time, wherein the molar ratio of the dropwise added sodium hydroxide to the urea is 1: 10;
D. accelerating the stirring speed after the dropwise adding is finished, continuously stirring for 2 hours, and then standing for 12 hours;
E. and (3) carrying out suction filtration on the solution after standing, washing a filter cake to be neutral by using deionized water, drying for 12h at the temperature of 80 ℃, taking out the filter cake, and grinding to obtain light yellow powdery hydrotalcite, namely the ethyl xanthic acid intercalation magnalium hydrotalcite.
2. The method for preparing the intercalated magnesium aluminum hydrotalcite of ethyl xanthic acid according to claim 1, wherein the method comprises the following steps: in the mixed solution A, the molar ratio of aluminum chloride to deionized water is 2: 25, and in the mixed solution B, the molar ratio of sodium ethyl xanthate to deionized water is 1: 40.
3. The method for preparing the intercalated magnesium aluminum hydrotalcite of ethyl xanthic acid as claimed in claim 2, characterized in that: in step C, the stirring speed is 120 rad/min; in step D, the stirring speed is 350 rad/min.
4. The method for preparing the intercalated magnesium aluminum hydrotalcite of ethyl xanthic acid according to claim 3, wherein the method comprises the following steps: in step D, the temperature of the solution at the time of standing was maintained at 40 ℃.
5. The method for preparing the intercalated magnesium aluminum hydrotalcite of ethyl xanthic acid as claimed in claim 4, wherein the method comprises the following steps: and in the step C and the step D, nitrogen is filled into the reaction container for protection.
6. The method for preparing the intercalated magnesium aluminum hydrotalcite of ethyl xanthic acid according to claim 1, wherein the method comprises the following steps: reaction vessel includes cavity (1), and the bottom of cavity (1) is provided with inclined plane (2), and the left side end on inclined plane (2) is higher than the right side end, and drip tube (3) are installed to the top of inclined plane (2) left side end, and the end-to-end connection of drip tube (3) has drip head (4) that a plurality of set up side by side, and stirring rake (7) are installed to the top of inclined plane (2) right side end.
7. The method for preparing the intercalated magnesium aluminum hydrotalcite of ethyl xanthic acid as claimed in claim 6, wherein the method comprises the following steps: a first heater (8) is installed on the side wall of the dripping pipe (3), and a second heater (9) is installed in the inclined plane (2).
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| CN102583347B (en) * | 2012-02-17 | 2014-05-07 | 北京化工大学 | Method for preparing graphene by using interlaminar two-dimensional confinement space of inorganic laminar material |
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| CN101293676A (en) * | 2008-06-12 | 2008-10-29 | 华东理工大学 | High specific surface area nanometer mesoporous cobalt-based spinel material and preparation method |
| CN101530621A (en) * | 2009-03-18 | 2009-09-16 | 北京化工大学 | Oxidation resisting dipeptide medicament intercalated houghite and preparation method thereof |
| CN102796280A (en) * | 2012-08-29 | 2012-11-28 | 北京化工大学 | Supramolecular intercalated structure polymer antioxidant |
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| CN108704603A (en) * | 2018-04-18 | 2018-10-26 | 中国科学院生态环境研究中心 | One step prepares method of the magnalium hydrotalcite nanometer sheet for adsorption and dephosphorization |
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